Apparatus for effecting chemical reactions



H. W. PA'ULUS.l

APP ARATUS FOR EFFECTING 'CHEMICAL REACTIONS.

APPLICATIONl FILED J'uLY 26,1920.

4 1,420,21 l Patented June 20, 1922 A 5 SHEETS-SHEET l- ""5 .C

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H. w. PAULus. APPARATUS FOR EFFECTING CHEMICAL REACTIONS.

APPLICATION FILED JULY 26, 1920.

' Patented June 20, 1922.

5 SHEETS-SHEET 3- H. W. PAULUS.

APPARATUS FOR EFFECTING CHEMICAL REACTIONS.

APPLICATION FILED JULY 26, |920.

Patented June 20, 1922.

5 SHEETS-SHEET 4..

i H. w. PAULUS. APPARATUS FOR EFFECTING CHEMICAL REACTIONS.

APPucATloN FILED JULY 26,1920.

Patented 311116 20, 192.2:

5 SHEETS-SHEET 5.

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` .HUMAN vwawfofo To all whom t may concern.;

` j miserie-s stares isa PAULUs, or RICHMOND HILL, NEW YoRE, AssIGNoR 'ro ROYAL EaxINef(y ECW'DER COMPANY, A CORPORATION' or NEW JERSEY.

HERMAN w.

APPARATUS' ECR EEFECTING CHEMICAL REACTIONS.

Y Application iled July 26,

Be it known thatfI, HERMAN PAULUS, a citizen of the United States, and a resi'- dent of Richmond Hill, in the county vof Queens and State of New York, have invented certain new and useful. Improvements in Apparatus for Effecting Chemical i Reactions, of which the following is a speciication.

The invention relates to apparatus for effecting chemical reactions by means of amalgams.

The object of the invention is to reorganize the construction and arrangement of parts of apparatus adapted for effecting chemical reactions, such as reductions, by means of amalgame, to the end that such reactions may be accomplished more effectively and more economically than is possible with the apparatus heretofore used for the pur-- pose. With this object in view, the invenj tion consists in certain novel improvements, constructions and arrangements, the advantages of'which vin securing the more effective and economical chemical reactions by means of amalgams will be pointed out as the description of the invention proceeds The preferred form of the invention Yis illustrated in the accompanying drawings in which Fig. 1 is a plan on a reduced scale of the improved apparatus for effecting chemical reactions by means of amalgame; Fig. 2 is a side elevation, partly in section,'of the electrolytic cell ;Figs. 3 and 4 are transverse sectional viewsA taken through the electrof lytic cell and the amalgam cooling trough at different points; Fig. 5 is a transverse section taken across the reduction chamber showing the mercury pump in' front elevation; Fig. 6 is a partial longitudinal section of the forward end of the reduction cham 'the apparatus with its accessory tanks and pumps for securing a continuous circulation of the electrolyte and the compound undergoing treatment. y

The apparatus illustrated in the drawings ...ser *e Eis-ffl Specification of Iietters Patent. Patented Jun@ 20, 19:22.

1920. serial No. 399,083.

. is adapted for efectin many kinds of chemical reactions in whic ployed. For the purpose of -illustrating the anv amalgam is emprinciples of the inventiomhowever, land to simplify the description, the apparatus lthe chamber to bring about the desired results; a mercury lift or pump 17 by which the mercury freed .from the amalgam is s. lifted or pumped back into the electrolytic cell; and a refrigerator or amalgam cooling,

trough 18 through which the amalgam passes from the electrolytic cell to the reduction chamber in order that it lmay be suiiiciently cool when it enters the reduction chamber.

of pregnant electrolyte through the electrolytic cell 15 the cell may be connected withy a tank 19 for containing the crystallized salts of the metal to be used for the amalgam. Sodium is taken for the sake of illus- .trationr-` lThe sodium chloride crystals are placed in the tank 19 to maintain the solution in concentrated or pregnant condition and the pum 2O raises the solution through the pipe 21 w ence it passes into the elevated end of the cell 15. The cell being arranged at an incline, the sodium chloride solution,"

which may now be termed the electrolyte,

flows through the cell and the impoverishedl electrolyte passes down the discharge pipe 22 into the tank 19 where it is again impregnated with the dissolved sodium chloride. The electrolytic action, of course, decomposes the sodium chloride into its component parts', the sodium-1 being dissolved in the 75 In order that there may vbe a circulation4 mercury to form the amalgam and thel chlorine passing down through the disAY Y charge pipe 22 and out through the chlorine discharge pipe 23.

` In order that there may be a circulation ofthe compound undergoing treatment in the reduction'chamber 16, 'a tank 25 is provided from which a pump 26 pumps the compound through a pipe 27 into the reduction chamber. The overflow from the reduction Chamber passes through the pipe 28 back into the tank 25. The circulation .of

the compound through the reduction chainber is continued until the desired reaction has been accomplished. 1n order that the operation of the apparatus may be continuous two tanks 25 may be provided. 1n the present instance, the chemical compound in the tanks 25 will be a mixture of oXalic acid, hydrochloric acid and water.

r1`he electrolytic cell 15 has a cast iron bottom or plate 30, accurately machined on its upper surface 31 so that the mercury may flow in an even sheet without the formation of pools and pockets. 1t has been found that the flow of the mercury is facilitated `by dividing the surface of the bottom 30 into separate longitudinal. channels 32 (Fig. 3) by means of tile orv porcelain blocks 33 inserted in longitudinally arranged pockets in the bottom 30. The number vof channels 32 will, of course, depend upon the size of the cell 15 and the conditions of opera'- tion. F our channels 32 are shown. The sides 35 and the ends 36 ofthe cell are of concrete blocks lined with tiles 37 inserted in recesses in the bottom 30. An open framework 38 of concrete constitutes the upper edge of the cell. The parts just described are all fastened together by bolts 39, which are properly insulated by dielectric bushings. The tiles 37 constitute insulators and prevent short circuiting between the electrodes. lnasmuch as a slight suction is maintained in the cell forl carrying off the chlorine gas the cell is covered with asbestos boards40 to prevent the infiltration of air. rlhe cell may be supported in any convenient manner as by the adjustable legs 46.

rlhe mercury 41 acts as the cathode. The iron bottom of the cell constitutes a convenient means for conducting the negative electricity from the mercury cathode. The cathode bus bar 42 is connected with the iron bottom of the cell by means of plates 43 secured to the bottom of the cell by studs 45.

The anodes may be of any suitable material and in the present instance are shown as slabs of graphite 47 resting on the tile blocks 33 and 37. Cylindrical leads 48 threaded at their lower ends screw into the an'ode slabs 47. The leads 48 pass through holes in a concrete beam 49'extending the length of the cell and resting on each end of the framework 38. The leads 48 are connected with an anode bus bar 51 supported from the beam 49 by means of uprights 52. The' ribbons v53 form electric connections between the leads 48 and the bus bar 51. r1`he positive current is conducted to the bus bar 51 through a lead 54.

It has been found in practice that the improved electrolytic cell described above is highly efficient in use. The combination of the iron bottom and the concrete walls permits a decrease inthe thickness of the mercury film and thereby effects a saving of ilaoaii that relatively expensive metal. Subdi-I viding the cell into longitudinal channels facilitates the flow of the mercury. The mercury enters the cell through the inlet opening 56 (Fig. 2). The mercury flows through the cell between the upper surface 31 of the bottom 30 and the lower surface of the anode slabs 47. rllhe electrolytic ac tion caused by the passage of the electriccurrent from 'the anodes 'to the mercury cathode splits up the sodium chloride in the cell and the sodium dissolves in the upper surface of the mercury and forms a coating of sodium amalgam thereon. The mercury and the sodium amalgam flow out of the cell through a discharge pipe 57 1t will be noted that a weir 58 is provided above the opening of the discharge pipe 57. 1t was found by having the orifice of the discharge pipe 57 flush with the surface of the bottom/ 30 of the cell that the amalgam tended to back into the cell and did not flow down through the pipe 37 with the mercury. .By providing the trough or weir 58 the tendency is for the amalgam to mix with the mercury as the two iow over the edge 59 of the weir and thus prevent the amalgam from backing up in the cell. This feature of construction conduces to the efficiency of the apparatus.

The electrolytic action in the cell 15 raises the temperature of the electrolyte and of the amalgam and mercury. Before the amalgam and, mercury enter the reduction chamber 16 to effect the desired chemical reactions it is necessary to reduce their temperature. F or this purpose they are passed through a refrigerator or amalgam cooling trough 18. The refrigerator or amalgam cooling trough is in the form of a tank 60, preferably composed of cast iron and having a double bottom forming a series of passage ways 61 through which the cooling fluid flows. The cooling fluid enters the channels 61 through the inlet pipe 62 and is charged through the outlet pipe 63. The amalgam and mercury enter the tank 60 throughI the discharge pipe 67 from the electrolytic cell yand are discharged through the pipe 64. It is thusseen that the amalgam and mercury and the cooling fluid flow in opposite direction so as to obtain the maximum cooling effect of the cooling liquor. Theupper surface 66 of the bottom of the trough 60 is properly machined so as to secure the flow of the mercury lin a thin sheet. It has been found desirable to provide the surface 66 with tranverse slots or depressions 67 by which the flow of the mercury is assisted by preventing the formation of pools and agglomerations. The vtrough 60 is enclosed in a framework of wood and the whole construction is supported by bolts 67 rising from angleirons 68 projecting outwardly from the cell is shown exaggerated in Fig. 11. rlhe discharge end of the trough 60 is also provided with a Weir 69 So as to prevent theamalgam from building up and being retained in the trough. A series of hinged-covers 69 close the top of the trough 18 and proyide ready access to its interior.

' through the pipe 64 into the reduction chamber 16. The reduction chamber consists of a rectangular concrete tank lined on its bottom and sides with acid proof material 71. To eect the roper Contact between the amalgam and the chemical compound to be reduced, the interior of the tank is subdivided into a series of longitudinal passages or channels 72 formed by acid proof walls 73. lin the present inst-ance there are sinv channels, three o-f which are receiving channels and three of which areV discharging channels. rlhe amalgam and mercury enter the receiving channels 74 thrugh inlet pipes 75 connected with the pipe 64. When the amalgam and mercury enter and leave the reduction chamber'they flow in the directions indicated by the arrows in Fig. 1. By causing the amalgam and mercury to flow in two directions in this manner a more. compact structure is produced. By the time the mercury bearing the amalgam on its surface has passed through the inlet channels 74 and the outlet channels 76 the sodium amalgam Contact with theacid thereby forming caustic soda and liberating hydrogen which. in its nascent state combines with the oXalic acid solution and reduces it to sodium glyoxylate. The mercury freed from the amalgam is discharged from the reduction chamer through the outlet pipe 77 into the pipe 78 whence it flows into the lower part of the merucy lift or the pump 17.

-The passage of the mercury and -the amalgam through the channels in t-he reduction chamber is effected by a series of paddle wheels 8O mounted on shafts 81 and journalled in'blocks 82 mounted on the sides vof the reduction chamber. Thereare two sets of the paddle wheels 80, one set. located in the inletchannels and the other set being located in the outlet channels. These two sets of paddle wheels, as is obvious, turn in opposite directions, and for this purpose each shaft 81 is rovided with a bevel gear which meshes wit corresponding bevel inion 84'secured to a shaft 85 iournale in -The cooled amalgam and mercury' flo-w has been acted upon by the aXolic acid and` hydrochloric acid solution in the chamber. 1 The amalgam is decomposed on coming in" lmercury in the bottom of the casi brackets 86 securedto one side of the reduction chamber. The shaft 85 is driven from a suitable source of power. The ends of the paddles dip into depressions 88 (Fig. 6) formed in the bottom of the reduction chamber. The depressions 88 are provided so that the mercury therein is scooped out and given a proper impulse to flow in a thin sheet toward the outletholes. At the same time that the mercury and amalgam are caused to ow through the channels in the reduction chamber the acid solutiogi is caused to fiow through the channels. rlhe acid solution, however, being of much less specific gravity than the mercury fio-ws -much faster. This is desirable so that the free acid lmay act upon the amalgam to decompose .it by the `time it reaches' the discharge openings.

Moreover, a constant circulation of acid solution is maintained through the reductionr85. chamber as described above so that the lib-4 erated hydro-gen may be taken up by the constantly changing solution of oxalic acid. The reduced solution goes down through the pipe 28 and the new solution enters through' 90 pipe 27.

rl`he bottomA of the reduction chamber is below the bottom of the electrolytic cell so that the mercury must be raised from the reduction chamber into the electrolytic cell. it is well kno-wn that mercury is a difficult substance to-handle properly'. Where centrifugal pumps are employed for conveying mercury from one level to another the mercury has a tendency to form colloids and to subdivide into minute globules which have a tendency to float on the surface of the solution, probably because of entrained air. One of the features of the present invention is to provide a lift or pump for raising the mercury from the lower level of the reduction chamber to the higher level of the electrolytic cell with a minimum of agitation of the mercury. The construction of this mercury pump is clearlyshown in Figs. 7 and 8. 110

The pump consists of a series of buckets 90 circularly arranged on the periphery of a plate 91 provided with a hub 92 secured to a shaft 94, which is journalled in a hub 95 projecting rearwardly from the casing 96 of 115 the drum. Each bucket 90 isI provided with a narrow slot 97 opening inwardly. This slot 97 serves as an inlet orifice and an outlet orifice. The buckets 90 rotate in the direction indicated by the arrow in Fig. 7. Power is supplied by.a worm gear 98 keyed to the shaft 95 and meshing with a worm 99 mounted on the shaft 85. The mercury enters the bottom of the casing 96 throughthe pipe 78. The levelof the mercury in the re- 125 duction chamber is indicated at 100 in Fig.

7. As the revolving buckets 90dip into the l 96 the mercury flows into the buckets th ough the orifices 97. Inasmuch as the orifices 97 are 1 30 located at the end of the buckets; toward the direction of travel, the mercury* does not flow out until the buckets are substantially at the top. rlhey empty or discharge into a receiving. trough 101 which discharges vthrough an opening 102 (Fig. 8) into a conduit 103 which discharges intol the upper end of theelectrolytic cell. Access is had'to the interior of the pump through a hingedcover 104.

rlhe mode of operation of the improved apparatus described above for effecting chemical reactions by means of amalgams lhas been given in connection with thev construction and operation of each of its component parts. It will be understood that the invention is not to be restricted to the form shown in the drawings, inasmuch as the principle of the invention may be embodied in other forms within the scope of the following claims.

k Having thus described the invention what is claimed as new is 1. An apparatus for` use in effecting chemical reactions by means of amalgame, comprising an electrolytic cell in which the amalgam is formed, said cell being divided into a series of longitudinal channels for facilitating the passage of the mercury therethrough, a chamber in which the chemical reaction takes place, a cooling trough between the cell and the chamber, the bottom of said trough ha ving a series of transverse depressions to facilitate the passage of the mercury therethrough, said chamber being divided into a series of channels into some of which the mercury passes from the trough -into the chamber and from some of which the mercury passes from the chamber into the cell, a series of paddles in the chamber for impelling the mercury in one direction and a second series of paddles in the chamber for impelling the mercury in the opposite direction, and means for returning the mercury from the chamber to the cell.

2. An apparatus for use in e'ecting chemical reactions by'means of amalgams, comprising an electrolytic cell in which the amalgam is formed, said cell being divided into a series of longitudinal channels for facilitating the passage of the mercury through the cell, a chamber in which the chemical reaction takes place, means for conducting the mercury and amalgam from the cell to the chamber, said chamber being divided into a series of longitudinal channels through which the mercury and amalgam flow, said channels being arranged so that the mercury and amalgam flow in one direction through some of them and in opposite direction through others, a Series of paddles in one set of channels for impelling the mercury and amal am in one direction, a second series of pa dles in the other set of channels for impelling the mercury and amalgam in the opposite direction, and means for returning the mercury from the chamber to the cell.

3. An apparatus for use in effecting chemical reactions by means of amalgams, comprising an electrolytic cell, a reduction chamber, connections between the cell and the chamber permitting mercury to flow from the cell to't-he chamber7 and means for lifting the mercury from the chamber into the cell, said cell being divided into a series of channels to facilitate the flow of the mercury therethrough.

4. An apparatus for use in effecting chemical reactions by means of amalgams, comprising an electrolytic cell in which the amalgamv is formed, a reduction chamber in which the chemical reaction takes place by means of the amalgam, and a trough interposed between the cell and the chamber for cooling the amalgam and the mercury before they enter the reduction chamber..

5. An apparatus for use in eecting chemical reactions byV means of amalgams, comprising an electrolytic cell in which the amalgam is formed, a reduction chamber in which the chemical reaction takes place and connections between the cell and the chamber, said cell being divided into a vseries of channels to facilitate the flow of the mercury therethrough and having at its discharge end a substantially perpendicular wall and a relatively sharp edge over which the amalgam and mercury fall to cause the amalgam and mercury to mix as they flow out of the cell.

6. An apparatus for use in effecting chemical reactions by means of amal ams, comprising an electrolytic cell in whic the amalgam is formed, a chamber in which the chemical reaction takes place, and connections between the cell and the chamber, the y cell being substantially rectangular in form and having at its discharge end a depression, one Wall of which is substantiallyperpendicular and having a relatively sharp edge over which the amalgam and mercury are caused to fall so that they will mix -as they How out of the cell.

7. An apparatus for use in effecting chemical reactions by means of amalgams, comprising an electrolytic cell in which the amalgam is formed, a chamber in which the chemical reaction takes place, connections between the cell and the chamber, said chamber being divided into a series of longitudinal passages through which the mercury and amalgam How, and means arranged wit-hin the chamber for causing the flow of the mercury and amalgam through the chamber.l

8. An apparatus for\ use in effecting comprising an electrolytic cell in which the nahmen' amalgam is formed, a chamber which the chemical reaction takes place, and connections between the cell and the chamber, l

the flow of the `mercury 'and amalgam` through the channels'.

9. An apparatus for use in effecting chemicalreactions by means of amalgame, comprising an electrolytic cell in which. the

amalgam is formed, a chamber in'which thechemical reaction takes place, connections between the cell and the chamber, said chamber being divided into a series of channels through which the mercury and amalgam How, revolving paddles 'located in the channels for impelling the flow of the mercury and amalgam, and depressions in the bot,

toms of the channels below the paddles into which the paddles dip. l

10. An apparatus for use in effecting chemical reactions by means of amalgams, comprising an electrolytic cell in which the amalgam 1s formed, a chamber in which the chemical reaction takes place, connections between the cell and the chamber consisting of -a cooling trough by whichthe mercury and amalgam are cooled before entering the chamber, said trough having a metal bottom with transverse grooves inthe surface thereof to facilitate the flow of the mercury therethrough.`

1l. An apparatus for use in effecting chemical reactions by means of amalgame,

comprising an electrolytic cell inf'which the amalgam is formed, a chamber in which the chemical reaction takes place,y means by which the mercury and amalgam lflow from the cell into the chamber, and means by which the melcury is returned from the chamber to the cell, saidl last named means comprising a series of rotating buckets having a single in let and discharge opening, connections between the chamber and the buckets to fill the buckets, and connections between the buckets and the cells through which the buckets discharge their contents into the cell,`

12. An apparatus for use in` effecting chemical reactions by means of amalgams,

comprising an electrolyticcell in which the.

' amalgam is formed,- achamber in'whioh the chemical reaction takes place, means throughl l which the mercury and amalgam flow from;

the cell into the chamber Aand .a pump v-for raisin "the mercury from. the chamber into the cel, said ery of a plate, said buckets having 'a single aperture which serves asl an inlet and an out ump consisting of a series 'of rotating buc I ets arranged on the periph' pump by which the mercury flows into lthe l buckets, and connections between the cell and the pump by which the mercury flows from the buckets into the cell.

13. An apparatus for use in eHecting chemical reactions by means of amalgams,

comp-risingan electrolytic cell in which the. f

amalgam is formed, a chamber in which the chemical reaction takes place, means by which the mercury and amalgam flow from the cell into the chamber, anda pump for raising the mercury from the chamber to Ithe cell7 said chamber consisting of a series of buckets arranged on the periphery of a plate, said buckets having each a single orilice arranged at 'its inner side, a pipe con. nection between the chamber and the pump having its discharge opening located above the orifices of the buckets when they are lat the lowest in their rotation, 4and means for 'receiving the mercury from the buckets and conducting it to the,A cell.

14:. AnV apparatus for use" in leffecting chemical reactions by means of amalgams, comprising an electrolytic cell in which the amal am is formed, a chamber in whichthe means for conducting the mercury from the buckets to the cell. p

15. An' apparatus for use in effecting lchemical reactions by means of amalgams, comprising an electrolytic cell in which the amalgam is formed, a chamber inwhich the chemical reaction takesplace, ,connections by which the mercury and amal am flow from the cell into the chamber, an a pump for returning the mercury from the chamber to the cell, said pump consisting of a casing into the lower part of which the chamberl discharges the mercury, a series of buckets arrangedvon theperiphery of a plate, means 'for rotating the plate so that the buckets will dip into the mercury at the bottom of the casing, each'bucket having on its inner side an orifice through which the mercury .in the bottom of the casing passes into the buckets, and a conduit between the. casing and the cell into which the buckets discharge kthe mercury during their rotation.

chemical reaction takesl \place, means lby h which thev lmercury and amalgam flow from the cell into the chamber, and .a pump for.-

etlll'nng the. mercuryv fromthe chamber to (c5 f ingenti `the cell, said pump comprising a circular between the chamber and the pump, and bep1ate,a series of buckets arranged on the petween the-pump and the ceH7 said buckets riphery of the plate, each bucket having a receiving the mercury at the lowest point in l0 f single orifice at its inner side, said oriee betheir cycle of rotation and discharging it ing locatedl at the end of the bucket toward at the highest point in their cycleof rotation. the direction in which the buckets rotate,

means for rotating the plate, connections HERMAN W. PAULUS. 

